Journal of ASTM International, Vol. 4, No.

8
Paper ID JAI100938
Available online at www.astm.org

Eric Fitamen,1 Laurent Tiquet,1 and Mathias Woydt2

Validation of Oxidative Stability of Factory Fill and

Alternative Engine Oils Using the Iron Catalyzed Oxidation
Test
ABSTRACT: Oxidation resistance is one of the limiting factors for long drains, bionotox, LowSAP or NoSAP
engine oils. The French iron catalyzed oxidation test ICOT uses 60 ppm iron acetylacetonate as diluted
catalyst under an aeration of 10 L/h at 170C. The ICOT ranks the oxidation stability of oils according to
three properties: a. the viscosity increase e.g., max. 40C100 % or 100C100 %, b. the increase to
an individual TAN e.g., max. 7.5 mgKOH/g and c. the oxidative evaporation losses of max. 10 % at
100 % due to oxidation. This paper describes the ICOT method standardized as GFC Lu 36T 03 and
the obtainable accuracy. Also, results are compiled achieved with this test for factory fill engine oils as well
as alternative prototype engine oils based on esters, blends of esters with hydrocarbons, and polyglycols.

Introduction
In order to reduce the costs related to testing and to meet the shortened development time schedules,
especially OEMs are more and more interested in methods which do not require an engine for testing
functional properties of lubricants and piston ring/liners materials/coatings. Recently, an increasing number of criteria have been placed for the engine oils to meet. This continuously reduces the time available
to address the new demands and turn them into functional solutions.
Most lubrication applications expose lubricants to oxygen in some manner. They are therefore susceptible to oxidation and, in the case of usage as engine oils, are additionally subjected to NOx and SOx.
In general, the purpose of oxidation testing is to study, evaluate, and meaningfully rank the oxidation
as well as the thermal performance of lubricant additives, base oils, and candidate formulations under
simulated operating conditions with the aim to predict as close as possible the performance of those
lubricants in real world applications.
A number of oxidation and thermal stability tests suitable for engine oils have been developed by
ASTM, DIN, JASO, IP, and French GFC:
a. ASTM D 4742 AFNOR NF T 60-182, Standard Test Method for Oxidation Stability of Gasoline Automotive Engine Oils by Thin-Film Oxygen Uptake, thin film oxygen uptake test
TFOUT,
b. DIN 51352, Testing of lubricants; determination of aging characteristics of lubricating oils;
increase in Conradson carbon residue after aging by passing air through the lubricating oil,
c. IP 48, Oxidation characteristics of lubricating oils,
d. ASTM D 6335, Standard Test Method for Determination of High Temperature Deposits by
Thermo-Oxidation Engine Oil Simulation Test, thermo-oxidation engine oil simulation test
TEOST,
e. CEC L-48-A-00, Bulk oxidation test same as GFC T-021-A-90,
f. JSAE JASO M333, High temperature oxidation stability test procedure for evaluating automobile gasoline engine oils, or
g. ASTM D 7098, New Standard Test Method for Oxidation Stability of Lubricants by Thin-Film
Oxygen Uptake TFOUT1 Catalyst B2.
Manuscript received December 4, 2006; accepted for publication June 18, 2007; published online September 2007. Presented at
ASTM Symposium on Automotive Lubricant Testing and Additive Development on 35 December 2006 in Lake Buena Vista, FL;
S. Tung, Bernard Kinker, and Mathias Woydt, Guest Editors.
1
RENAULT SAS, F-78288 Guyancourt
2
Federal Institute for Materials Research and Testing BAM, D-12200 Berlin
Copyright 2007 by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.
Copyright by ASTM Int'l (all rights reserved); Thu Sep 2 14:44:46 EDT 2010
Downloaded/printed by
National Institute of Technology Surat Gujarat State pursuant to License Agreement. No further reproductions authorized.

2 JOURNAL OF ASTM INTERNATIONAL

FIG. 1Schematics and photos of the test equipment used for the ICOT.

It has to be noted, that many companies have proprietary methods they use in-house. The French GFC
standardized ICOT developed by the GFC working group LM2/SG6 can be considered as an OEMdriven in-house test of the two French car makers, Renault SAS and PSA Peugeot Citron, with a clear
emphasis on car engines, which actually attracts the attention of other European car manufacturers.
Other OEMs, like FORD with the FOAT 1 Ford Oil Aging Test, developed also a proprietary
engine oxidation test which reflects the OEMs-specific needs. FOAT intends to simulate the ASTMsequence IIIE and is suited for the homologation of engine oils according to the FORD Double IIIE
specification. The viscosity increase was limited to +50 % after 128 h.
The ICOT is attractive overall for benchmarking factory fill oils of competitors and suppliers as wells
as ranking alternative engine oil concepts prior to engine testing. Basically, the combined intrinsic functional properties of ICOT are its valued attraction.
Test Method
Apparatus
The French ICOT 2 ICOT= iron catalyzed oxidation test, see Fig. 1 uses 60 ppm iron acetylacetonate
C15H25FeO6 as the diluted catalyst. The initial amount of oil needed is 150 g, with air bubbling through
this specimen at a rate of 10 L / h for a period of test time which is a function of the oil performance
expected usually 0, 12, 24, 48, 72, 96 h, etc.. In order to perform an ICOT with a duration of 96 h, six
tubes are needed.
Drain Criteria (Oil Changes Intervals)
The ICOT defines the oxidation resistance of a lubricant at 170 C under an aeration of 10 L / h for three
properties: viscosity, TAN, and oxidative evaporation loss. A lubricant is considered to have reached the
end of its lifetime or lost its resistance to oxidation, if:
The viscosity increase is larger than e.g., 100 %,
1. the increase of an individual TAN exceeds 7.5 mgKOH/ g and or?
2. the oxidative evaporation losses at = 100 % exceed 10 %. The actual times for these three
properties of a lubricant tested to reach the above conditions may differ, but all three give a quite clear
indication about the oxidation processes. The oxidative evaporation losses should not be higher than 10%
at the criteria of a viscosity increase of = 100%.
The induction times of the ICOT properties can differ among the OEMs, e.g., 50 to 200 % for the
viscosity increase at 40 or 100 C. The ICOT indicates only the oxidative resistance and gives no hint
about the AW/EP-retention of a formulation. For actual factory fill oils, one ICOT hour corresponds to
Copyright by ASTM Int'l (all rights reserved); Thu Sep 2 14:44:46 EDT 2010
Downloaded/printed by
National Institute of Technology Surat Gujarat State pursuant to License Agreement. No further reproductions authorized.

FITAMEN ET AL. ON USING THE IRON CATALYZED OXIDATION TEST 3

TABLE 1Accuracy Statements for the French ICOT (7 Co-operators).
Precision statement from RR tests
Repeatability
Reproducibility

r = 0.05 H
R = 0.15 H

or 96 h 5 h
or 96 h 15 h

Note: H is the interpolated hour with % increase of the chemical characteristic.

270 330 km of driving. This relation has to be validated for esters and polyglycols. The ICOT life of
PCMO based on hydrocarbons for a drain of 30 000 km lies around 100 hours.
Accuracy of ICOT Results
In order to assess the accuracy of the ICOT, the philosophy of the French working group is to actually use
the duration option for comparison. Although the duration of ICOT exceeds other tests by far, its results
are more representative than calculating the respective accuracy based on a one-hour test only. After one
hour, the lubricant is still far from the end of its lifetime which, however, is the best condition to appreciate
the accuracy of the method see Table 1.
Results
Factory Fill Oils
Comparing Fig. 2 with the experiences gained in the field with the test results obtained with the ICOT, the
following extrapolations can be made:
a. ACEA A2/B2 classified lubricants have an ICOT lifetime below 48 h which converts to a maximum oil change interval of 20 000 km,
b. ACEA A3/B3 ones have an ICOT lifetime between 48 and 72 h converting to an oil change
interval of between 20 000 and 30 000 km,
c. ACEA A3/B3 high performance grades exhibit an ICOT lifetime between 72 and 96 h and have
a target oil change interval of 30 000 km,
d. ACEA A5/B5 grades have an ICOT lifetime above 96 h and a potential oil change interval of
40 000 km.

FIG. 2Viscosity increase versus oxidation test time T 170 C of different factory fill oils (red
curves ACEA A2/B2, blue curves A3 / B2 and A1/B1; green curves A5 / B5)
Copyright by ASTM Int'l (all rights reserved); Thu Sep 2 14:44:46 EDT 2010
Downloaded/printed by
National Institute of Technology Surat Gujarat State pursuant to License Agreement. No further reproductions authorized.

4 JOURNAL OF ASTM INTERNATIONAL

FIG. 3Viscosity increase versus oxidation test time T 170 C of different alternative oils and factory
fill oils.

Figure 2 suggests that the performance level of factory fill oils can be ranked semi-quantitatively by
the ICOT test. It is also interesting to note that some formulations display a loss or drop in viscosity which
is a concern for the hydrodynamic design of the tribosystems. Therefore, the viscosity increase as criteria
may also be put into relation to this drop in viscosity.
Alternative Oils
Figure 3 displays the viscosity increase versus test time and Fig. 4 the oxidative evaporation losses during
ICOT used for validation of alternative engine 3 oils the respective base oils used are esters, polyglycols
as well as blends of esters with hydrocarbons.
The GreenTec LS 100 % ester base oil as well as the best bio-no-tox formulations GT1 a blend of
hydrocarbons with esters, which conforms with VW 50300/ 50600, PPG 32-2 + Phopani or PAG 46-4

FIG. 4Oxidative evaporation losses of different engine oil formulations versus ICOT time T
170 C.
Copyright by ASTM Int'l (all rights reserved); Thu Sep 2 14:44:46 EDT 2010
Downloaded/printed by
National Institute of Technology Surat Gujarat State pursuant to License Agreement. No further reproductions authorized.

FITAMEN ET AL. ON USING THE IRON CATALYZED OXIDATION TEST 5

FIG. 5Evolution of TAN versus ICOT time of polyglycols.

+ Phepani achieves between 100 and 160 h of lifetime before reaching one of the criteria of the ICOT for
long duration. For convenience, the artificial names Phopani and Phepani are used as abbreviations for
the respective additive packages.
The custom-made polyglycols PPG32-2 and PAG46-4 with the proprieraty boosters for oxidation
resistance have an ICOT lifetime of at least 96 h respecting the bionotox-criteria biodegradable and
nontoxic. Overall, Phopani ensures 100 h and Phepani even 130 and more hours of lifetime.
The contribution of a properly selected polyglycol base becomes obvious by comparing the evolution
of the oxidative evaporation losses of the PAG 46-4 base oil b.o. to the additivated PAG 46-2. The PAG
46-4 base oil reached one of the drain criteria after 30 h. Further comparison reveals that the Papani- and
Phopani-package can stabilize viscosity increase for up to 100 h, but not the oxidative breakdown
resulting in excessive weight losses. In contrast, the Phepani-package in a proprietary polyglycol boosts
the respective lifetime up to 130 h concerning all three ICOT drain criteria, viscosity and TAN increase
as well as evaporation loss.
The PAG 46-4+ 2,6 Phepani achieved the same ICOT lifetime concerning the viscosity increase as the
ester-based Titan GT1 SAE 0W-20 Fig. 3 and exhibited the same evolution in oxidative weight loss see
Fig. 4. The evolution of the oxidative weight losses gives a good indication of the protecting effect of the
antioxidant package against breakage of the molecules of the base oil.
The custom made PAG 46-4 base oil in its unadditivated form reached the individually set limit of
7 mgKOH/ g for the TAN criterion after 48 h see Fig. 5. Adding 2.9 Phepani to the PAG 46-4, the
evolution of TAN over ICOT time impressively demonstrated that the set limit for the TAN criterion was
not passed after 130 h or even 192 h.
Even the candidates for ultra-long oil change intervals, namely Greentec LS 100 % ester and TOTAL
100E 100 % ester followed by the PAO-based formulation SAE 0W-30 SLX, exhibiting the lowest
oxidative weight losses after 200 h see Fig. 4, reached the drain criteria for TAN and viscosity earlier.
Conclusions
Without the need of engines, ICOT proves the feasibility to evaluate the oxidative stability within a
reasonable test time. Combining the three criteria viscosity increase, TAN, and evaporation loss, ICOT
allows a deep insight into the oxidation kinetics.
The new GFC method is the best way to screen the ACEA oil performances in relation to their on-road
performances. This test is discriminative to the entire range of engine oils and the information is available
in a short time. With this laboratory test, it is possible to extrapolate the oil change interval. However,
oxidation performance is only one parameter of oil degradation. The thickening observed after engine
Copyright by ASTM Int'l (all rights reserved); Thu Sep 2 14:44:46 EDT 2010
Downloaded/printed by
National Institute of Technology Surat Gujarat State pursuant to License Agreement. No further reproductions authorized.

6 JOURNAL OF ASTM INTERNATIONAL

testing is an additional effect also related to the volatility and soot intake of the oil. Also the dilution by
fuels.
The ICOT can also be applied in order to screen Low-/NoSAP, polymer, and metal-free alternative
engine oils in relation to their bionotox properties.

References
1

Korcek, S., Jensen, R. K., and Johnson, M. D., Assessment of Useful Life of Current Long Drain
and Future Low Phosphorus Engine Oils, Proceedings International Tribology Conference, September 2001, Vienna.
GFC Lu 36T 03, Test doxydation catalys par lactyle actonate de fer ICOT, Groupe Franais
de Coordination GFC, Le Consulat, 147, av. Paul Doumer, F-92852 Rueil-Malmaison, gfc@gfctests.org; see also IP48/97 Determination of Oxidation Characteristics of Lubricating Oil, 2004.
Desplanches, G., Criqui, B., Linnemann, T., and Woydt, M., Tribological Performances of New
Triboactive Ti,Mo C,N and Tin2Cr2O2n1 as Piston Ring and Cylinder Liner Coatings Interacting With Bio-no-tox Lubricants, Plenary paper at 15th Int. Coll. Tribology, TAE Esslingen, 1719
January 2006, ISBN 3-924813-62-0 or in Industrial Lubrication and Tribology, Issue 2, 2008.

Copyright by ASTM Int'l (all rights reserved); Thu Sep 2 14:44:46 EDT 2010
Downloaded/printed by
National Institute of Technology Surat Gujarat State pursuant to License Agreement. No further reproductions authorized.